EP2622112A1 - Vorrichtung und verfahren zum verdampfen von material aus einer metallschmelze - Google Patents
Vorrichtung und verfahren zum verdampfen von material aus einer metallschmelzeInfo
- Publication number
- EP2622112A1 EP2622112A1 EP12791755.7A EP12791755A EP2622112A1 EP 2622112 A1 EP2622112 A1 EP 2622112A1 EP 12791755 A EP12791755 A EP 12791755A EP 2622112 A1 EP2622112 A1 EP 2622112A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- crucible
- region
- molten metal
- crucible region
- susceptor
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 98
- 239000002184 metal Substances 0.000 title claims abstract description 98
- 239000000463 material Substances 0.000 title claims abstract description 65
- 238000001704 evaporation Methods 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims description 24
- 230000008020 evaporation Effects 0.000 title description 16
- 230000008569 process Effects 0.000 title description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 28
- 230000005674 electromagnetic induction Effects 0.000 claims abstract description 6
- 230000009471 action Effects 0.000 claims abstract description 3
- 239000012159 carrier gas Substances 0.000 claims description 29
- 239000000203 mixture Substances 0.000 claims description 10
- 230000008878 coupling Effects 0.000 claims description 8
- 238000010168 coupling process Methods 0.000 claims description 8
- 238000005859 coupling reaction Methods 0.000 claims description 8
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 7
- 229910052733 gallium Inorganic materials 0.000 claims description 7
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 6
- 229910052738 indium Inorganic materials 0.000 claims description 6
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 6
- 239000011364 vaporized material Substances 0.000 claims description 4
- 238000009792 diffusion process Methods 0.000 claims description 3
- 230000001939 inductive effect Effects 0.000 claims description 3
- 230000008016 vaporization Effects 0.000 claims description 3
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 2
- 230000001419 dependent effect Effects 0.000 claims description 2
- 239000003989 dielectric material Substances 0.000 claims 1
- 238000005192 partition Methods 0.000 claims 1
- 239000000155 melt Substances 0.000 description 32
- 239000007789 gas Substances 0.000 description 13
- 230000006698 induction Effects 0.000 description 13
- 230000005670 electromagnetic radiation Effects 0.000 description 11
- 238000002844 melting Methods 0.000 description 9
- 230000000694 effects Effects 0.000 description 7
- 230000005855 radiation Effects 0.000 description 7
- 230000008018 melting Effects 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- 150000002739 metals Chemical class 0.000 description 5
- 241000894007 species Species 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000011109 contamination Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000036961 partial effect Effects 0.000 description 3
- 230000035515 penetration Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000002207 thermal evaporation Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000002829 reductive effect Effects 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000007723 transport mechanism Effects 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000009529 body temperature measurement Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 230000005672 electromagnetic field Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 238000002202 sandwich sublimation Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/26—Vacuum evaporation by resistance or inductive heating of the source
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/228—Gas flow assisted PVD deposition
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/243—Crucibles for source material
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/246—Replenishment of source material
Definitions
- the invention relates to an inductively heated device for the thermal evaporation of material from a melt with high electrical conductivity (hereinafter molten metal or metallic melt) and a corresponding method.
- the device can be used as a material source for the production of coatings and materials in a wide pressure range from high vacuum to atmospheric pressure.
- the material of the molten metal may in particular also be the low-melting metals, such as e.g. Gallium, indium, aluminum or mixtures thereof.
- Evaporators are used predominantly under high vacuum conditions (Shah, S. et al., Supra, A. Kuzmichev et al., (2011), supra), with molecular flow being the dominant transport mechanism for the vaporized species.
- the evaporation also takes place in a rough vacuum and the transport in the gas phase by convection and diffusion (see: Yu. Vodakov et al., "High Rate GaN Epitaxial Growth by Sublimation Sandwich Method", J. Crys. Growth 183 (1998) 10, E. Berkman, PhD Thesis, North Carolina State University, 2005; M. Imade et al., Mat Lett. 59 (2005) 4026; H. Wu et al., Phys. Stat sol (c) 7 (2005) 2032; D. See et al., J. Crys. Growth 310 (2008) 916.
- the inductor can be found directly on the crucible (v. I. Arnes et al., "Crucible type evaporation source for aluminum", Rev. Sei, Instr., 37 (1966) 1737, RR Phinney, DC Strippe, "Crucible for v. Kuzmichev, L.
- the evaporation temperature can be adjusted by direct or indirect, electro-magnetic coupling between the melt and the inductor.
- the heat is induced directly in the melt with minimal losses. Strong Lorentz forces, however, often result in an unstable hydrodynamic situation, eg, with the occurrence of irregular fluctuations in the enamel surface (A. Kuzmichev et al. (201 1), loc.
- the indirect version is based on the decoupling of the heat in a susceptor fixed at working temperature.
- the susceptor functions either simultaneously as a crucible (I. Arnes et al., Loc. Cit.) Or susceptor and crucible are designed as separate components (RR Phiney et al., Supra, A. Kuzmichev et al (2008) , supra).
- the heat transfer to the melt takes place by means of heat conduction and radiation.
- Criteria for the selection of the susceptor material are a high melting point and a high electrical conductivity as well as a high resistance to thermal shock and the most inert behavior possible with respect to the melt and gas atmosphere present in the specific application.
- Preferred material is graphite (RR Phinney et al., Loc. Cit., A. Kuzmichev et al (2008), loc. Cit.), While conductive specialty ceramics (I. Arnes et al., Loc. Cit.) Or molybdenum (RR Phinney et al., Loc. Cit.).
- a major drawback to using a susceptor is that it is always a significant source of contamination in the system regardless of the material and embodiment.
- One aspect of the invention provides a device comprising a first crucible or crucible region and a second crucible or crucible region.
- the first crucible or crucible region is provided for receiving the molten metal to be evaporated
- the second crucible or crucible region is provided for receiving a susceptor material.
- the first crucible or crucible region and the second crucible or crucible region define spatially different interior spaces - one for receiving the molten metal and the other for receiving the susceptor material - these interiors may be separated according to one embodiment, but also interconnected according to another embodiment ( eg in the manner of a siphon).
- crucible is to be understood here as an independent container, while the term crucible region refers to a crucible or container-like section of a contiguous arrangement, which also comprises a plurality of individual components or walls. can be set. In particular, in this aspect such a common arrangement may comprise the two or more crucible regions.
- the molten metal may be the melt of any substance, in particular a metal.
- Particularly advantageous embodiments are achieved with regard to suitability of the crucible or crucible region (or the crucible or crucible regions) for melts of gallium, indium and / or aluminum.
- the suitability includes, among other things, the corresponding chemical, thermal and / or mechanical pressure resistance of the crucible or crucible region in relation to these substances.
- the susceptor material has the property of converting applied electromagnetic radiation into heat via induction.
- the susceptor material is the molten phase of the same or at least a similar material to that of the molten metal to be evaporated.
- the electromagnetic radiation to be converted into heat by induction is generated by a heating source so designated by virtue of this effect.
- the electro-magnetic radiation to be generated is a suitable radio-frequency or microwave radiation adapted for this purpose and preferably to the susceptor material, e.g. from the frequency range between 0.1 kHz and 300 GHz, other - especially adjacent - wavelength ranges are not excluded according to the embodiments.
- the heating source is now arranged with respect to the first crucible or crucible region and the second crucible or crucible region such that it seals the susceptor material in the second
- Crucible or crucible area due to electromagnetic induction heats up, while the molten metal in the first crucible or crucible area does not or only slightly heats up.
- “Irrelevant” here means that the heating of the molten metal due to the electromagnetic induction directly through the heating source is not sufficient to achieve the evaporation process or at least maintain.
- an effect of this arrangement is therefore that the first crucible or crucible region (or more precisely: the molten metal contained therein), for example, by the second Crucible or crucible region (or more precisely, by the susceptor material contained therein) or other means from the action of electromagnetic radiation or induction is shielded.
- the mutual arrangement of the two crucible or crucible regions with respect to the heating source plays a role here, as well as the effect that the electromagnetic radiation used has only a limited penetration depth.
- the heat required for the evaporation of heat is accomplished via a thermal coupling between the first and second crucible or crucible areas. It has been found that by this embodiment an otherwise occurring splashing of the molten metal at its surface can be avoided, which would take place if the molten metal were exposed directly to the magnetic induction.
- undesirable droplet formation can be at least reduced, if not eliminated altogether.
- a susceptor material provided in a second crucible or crucible region is provided and heat is supplied by inductive heating of the susceptor material. Further, a molten metal or a corresponding unmelted starting material is provided in a first crucible or crucible region connected to the second crucible or crucible region by thermal coupling. The heat is transferred by the thermal coupling from the susceptor material in the second crucible or crucible region to the molten metal in the first crucible or crucible region so that the molten metal reaches a desired temperature. The molten metal in the first crucible or crucible region is evaporated at the desired temperature.
- Fig. 1 shows a first embodiment of a device according to the invention for evaporating a molten metal.
- Fig. 2 shows a second embodiment of a device according to the invention for evaporating a molten metal.
- FIG. 3 shows a perspective sectional view of the device according to the second embodiment of FIG. 2.
- FIG. 4 shows a third exemplary embodiment of a device according to the invention for evaporating a molten metal.
- 5 shows a fourth exemplary embodiment of a device according to the invention for evaporating a molten metal.
- a first embodiment of a device according to the invention for evaporating a molten metal comprises a first crucible 103 and a second crucible 102. Further, a source 110 for heating and melting the material (eg, a powder) contained in the second crucible 102 is provided to form a melt 105.
- the material may be any metal. Metals-containing mixtures or metallic compounds are here likewise encompassed by the term metal.
- the material of the melt 105 may in particular also be low-melting metals, such as e.g. Gallium, indium, aluminum or mixtures thereof.
- the heating effect is effected in this non-limiting example by an electromagnetic radiation 115, wherein the source 110 may comprise, for example, a radio-frequency coil generating the radiation.
- the radiation or its wavelength or its wavelength spectrum is matched to the material of the molten metal 105, so that it heats up via electromagnetic induction.
- the molten metal 105 serves here correspondingly as a susceptor material.
- the induction power can be adjusted by control of the source 110. The maximum power is enough to melt the metal material.
- the crucible may be made of a nonconductive, thermally and chemically resistant, such as pyrolytically deposited boron nitride (pBN) or other suitable materials be formed, and is hereby closed by a cover 119 to prevent escape of the evaporating metal gas.
- pBN pyrolytically deposited boron nitride
- the first crucible 103 and the second crucible 102 are thermally coupled to one another via a heat coupling 112. It may be a material with high thermal conductivity, so that a melt 106, which is provided in the first crucible 103 and, for example, also the same or a similar material as in the melt 105 includes, in particular low-melting metals such. Gallium, indium, aluminum or mixtures thereof, etc., is brought to almost the same temperature as the molten metal 105 in the second crucible 102nd
- the shielding occurs because, viewed from the heating source 110, the second crucible 102 is arranged spatially in front of the first crucible 103 and the electromagnetic radiation 115 causing the induction 116 is absorbed by the molten metal 105 in the second crucible 102.
- the two crucibles 103 and 102 may also be connected by a conduit 114 which may serve to exchange between the two melts or to re-flow to replace vaporized melt in the first crucible.
- a refilling device for the material of the melt may also be provided on the second crucible (not shown).
- the metal vapor or the metal gas 109 is either collected according to this embodiment and carried in a transport line 111 by a carrier gas 108 to be supplied in a further desired use or removed in vacuum as a particle beam (without transport line 111).
- FIG. 2 shows a cross-sectional view of a second embodiment of a device for evaporating a metal from a melt with transport of the vaporized species in the gas phase through a suitable process gas stream.
- the materials intended for the melts 5, 6 provided here correspond to those of the first embodiment.
- the device is located in a quartz glass reactor 16, which is connected to a vacuum system (not shown) with which a defined working pressure between 1 and 1000 mbar can be set.
- a vacuum system not shown
- the invention is in no case limited to such pressure ranges and higher pressures are also possible.
- the device comprises a concentrically arranged, cylindrical, double-chamber crucible system in a vertical position with a first crucible region 26 and a second crucible region 25.
- the second crucible region 25 surrounds the first crucible region 26 in the form of a cylinder shell and shields it from the outside.
- the first crucible region 26 encloses a channel 28, which extends along the vertical axis of symmetry in this particular example
- the first crucible region 26 is connected to the channel 28 via an opening to discharge the vaporized material.
- the opening is in an annular region of the upwardly open first crucible region 26.
- the openings can of course also be directed laterally.
- the diameter of the openings can be arranged controllable from the outside.
- the first, inner crucible region 26 is formed in this embodiment by the wall of a downwardly open, funnel-shaped element 4 and by the inner wall 3 of the second, outer crucible region 25.
- the crucible may in turn consist of a non-conductive, thermally and chemically resistant, such as pBN or other suitable materials.
- a suitable refilling device eg a capillary (not shown in FIG. 2), vaporized material can be refilled in solid (eg powder) or liquid form.
- the refilling can be controlled according to a specific modification, wherein for example the weight of the illustrated double-chamber crucible system is monitored by means of a weight sensor (not shown in FIG. 2).
- the second crucible region 25 is formed by the crucible element 3 (inner wall), by the widening part of the inverted funnel-shaped element 4 (bottom) and by an outer crucible 2 (outer wall).
- the wall 3 common to the first and second crucible regions 25, 26 may include openings (not shown) to allow material exchange between the two crucible regions.
- the openings may be formed in particular in the lower region of the crucible or crucible regions in the manner of a siphon, in which case the melt surfaces in the two crucibles are the same height.
- the second crucible region 25 an identical or a similar molten metal (susceptor 5, for example a metal of a similarly low melting point) is introduced as in the inner crucible region 26.
- the second crucible region 25 is closed at the top by a cover 27 to prevent the evaporation of the material.
- the bore 34 which is otherwise closed with the screw 35, is located in the cover.
- a heating source 10 in the form of a radio-frequency coil is arranged outside the quartz glass reactor 16.
- the coil (heating source 10) generates a radiation tuned to the molten metal of the outer crucible region 25, so that it can be heated by induction.
- Crucible region 26 thus acts as a susceptor 5 for the electromagnetic radiation.
- the thickness of the susceptor ie the inner distance between the crucible elements 2 and 3 of the outer crucible region is greater than the penetration depth of the electromagnetic radiation of the radio-frequency coil (heating source 10). This ensures that the molten metal 6 in the inner crucible region 26 is not or not significantly influenced by the radiation of the coil. Rather, the melt 6 in the inner crucible region 26 is heated by heat conduction from the second crucible region 25 via the wall of the crucible element 3. Due to the concentric arrangement of the crucible regions, the interface between the crucible regions 25, 26 is particularly large in relation to the volume content, which promotes efficient heat transfer.
- the crucible material of the crucible element 3 must allow the heat transfer, which is e.g. given when using pBN.
- the invention is not limited to this selection of materials.
- the temperature in the molten metal (susceptor material 5) and / or in the molten metal 6 can be determined by means of thermocouples (not shown in FIG. 2), which, according to a modification of the exemplary embodiment, form a control circuit together with the heating source 10, around the melt to keep at a desired temperature.
- An advantage of this construction is that negative effects of the electromagnetic fields associated with the induction heating, such as spraying or droplet formation on the surface of a melt, are limited to the outer, closed crucible region 25.
- the molten metal in the inner crucible region 26 can evaporate stably and homogeneously without droplet formation, which represents an essential prerequisite for improved quality of the subsequent processes.
- the limited by the crucible 4 of the inner crucible central channel 28 is traversed by the carrier gas 8.
- the carrier gas 8 is used to adjust the total pressure in the reactor 16 and the transport and dilution of the metal species vaporized from the melt stock 33 of the inner crucible region 26 in the gas phase.
- the carrier gas 8 can be formed from any desired inert gas, for example argon, hydrogen, nitrogen or suitable mixtures of inert gases. Depending on the flow direction of the carrier gas 8 axially upward or downward, the vaporized metal species are transported up or down out of the crucible system area. The possible flow directions of the carrier gas 8 are indicated in FIG. 2 by the double arrow. In addition to the total pressure in the reactor, the carrier gas flow 8 represents a further essential parameter for the flexible adjustment of the transport rate and direction of the vaporized metal species in the system.
- the funnel shape of the crucible element 4 delimiting the channel 28, together with a suitably selected, constant flow velocity, enables a substantially vane-free carrier gas flow and thus a stationary transport of the vaporized metal species with a constant transport rate, which in turn constitutes an essential prerequisite for an improved quality of the subsequent processes.
- the device according to the second embodiment is not limited to the geometry of the crucible 4 shown in FIG. Other geometries are also possible, provided that the laminar character of the gas flow 8 is maintained.
- FIG. 3 shows a perspective view of the double-chamber crucible system shown in cross-section in FIG. 2 and described above for illustrating the concentric arrangement of the crucible elements.
- the inner crucible region 26 bounded by the crucible elements 3, 4 with the molten metal 6 to be vaporized.
- the crucible element 4 also delimits the central channel 28 for the axially upward or downward flow of the carrier gas 8.
- the outer crucible region 25 susceptor 5
- the inner crucible region 26 is also filled with the material to be evaporated in powder form or as granules.
- a radio-frequency coil as heating source 10
- the material Due to the induced heat, the material is heated above the melting point, so that the molten susceptor 5 is formed.
- the heat generated in the outer crucible region 25 is transferred by heat conduction and radiation to the metal in the inner crucible region 25, as a result of which this likewise heats up above the melting point and is present as melt 6.
- the molten metal 6 will partially evaporate, the rate of evaporation or saturation partial pressure being defined by the temperature of the susceptor melt after adjustment of the temperature balance between the crucible regions 25, 26.
- the minimum temperature for the operation of the device is determined by the melting points of the materials (susceptor 5, molten metal 6).
- the maximum operating temperature is determined by the thermal stability of the crucible material and is, for example when using pBN above 2000 ° C.
- the flow of a carrier gas 8 or a carrier gas mixture with a defined mass flow from one or more external gas sources is generated and directed axially upwards or downwards through the central channel 28 of the device.
- the metal vapor of the melt 6 formed in the inner crucible region 26 mixes with the carrier gas or the carrier gas mixture by diffusion processes.
- the metal vapor of the melt 6 is removed from the device either upward or downward as a result of convection processes and fed to a further use.
- stationary transport of the metal vapor through a laminar flow of carrier gas is essential.
- FIG. 4 shows in a cross-sectional view a third embodiment of an apparatus for evaporating a metal from a melt with transport of the vaporized species under high vacuum conditions.
- the device is located in a vacuum chamber made of stainless steel or other vacuum-resistant material (not shown) which is connected to a vacuum system (not shown) to which a pressure of less than 10 "4 mbar can be set.
- the apparatus comprises a concentrically arranged, cylindrical, double-chamber crucible system in a vertical position, which analogously to the second exemplary embodiment (FIG. 2, 3) comprises an outer crucible region 26 with the melt 5 functioning as a susceptor and an inner crucible region 25 with the molten metal 6 to be vaporized consists.
- the outer crucible region 26 is formed in this embodiment by a cylindrical crucible with a closed bottom 2, by a cylindrical crucible 3 open on both sides with a smaller diameter than the crucible 2 and by a circular cover element 27.
- the lid member includes a bore 34 which can be closed with a screw 35.
- the inner crucible region 25 is bounded laterally and downwardly by the inner crucible element 3 and the bottom of the crucible element 2.
- the structure of the heater i. the coil as a heating source 10 (not shown in FIG. 4) corresponds to the arrangement shown in FIG. 2, whereby here too the symmetry axes of the coil and the crucible or crucible regions can preferably coincide.
- the heating of the crucible system up to the setting of a defined partial pressure of the species evaporated from the molten metal 6 corresponds to the principles described in detail in the second embodiment (FIGS. Furthermore, the statements made for the second exemplary embodiment regarding the selection of the materials (susceptor 5, melt 6) and for the crucible elements also apply without restriction to the third exemplary embodiment described here.
- a carrier gas stream in the process chamber is dispensed with.
- the crucible system has no central channel, but is limited down through the bottom of the crucible element 2. The vaporized metal is transported away under high vacuum conditions by the molecular flow from the region of the evaporation source upwards and supplied for further use.
- Fig. 5 shows a perspective view of a fourth embodiment of a device for evaporating a metal from a melt in a horizontal arrangement.
- Such elements approximately corresponding to the preceding embodiments are here provided with the same reference numerals.
- the device is located in a quartz glass reactor (not shown), which is connected to a vacuum system (not shown) with which, just as in the second embodiment (Fig. 2, 3), a defined working pressure between 1 and 1000 mbar can be set.
- a quartz glass reactor not shown
- a vacuum system not shown
- the invention is in no case limited to such pressure ranges and higher pressures are also possible.
- the apparatus comprises a horizontally arranged dual-chamber crucible system comprising an upper crucible region and a lower crucible region.
- the upper crucible region is formed in this embodiment by a container 2a having a rectangular cross section and a matching lid 27.
- the lower crucible region is formed by a further container 2 with a rectangular cross section and a matching lid 3.
- the cover elements 3, 27 contain openings 34 for refilling purposes, which can be closed with screws 35.
- the opening 34 can also be used for temperature measurement during the process.
- an extended recess is formed, which comprises a majority of the entire bottom surface.
- a recess for recessing the upper container bottom is formed in the cover element 3 of the lower crucible container 2.
- the crucible containers 2, 2 a serve to receive the susceptor material 5.
- the metal to be evaporated (molten metal 6) is introduced into the depression of the cover element 3 of the lower crucible container 2.
- rectangular recesses are present, so that in the arrangement of the crucible elements of FIG. 5 results in a flat, horizontal channel 28 with a rectangular cross-section between the upper crucible container 2a and lower crucible container 2.
- the high frequency coil not shown in FIG. 5 as the heating source 10 has a (in the reference system of the figure) vertically extending axis of symmetry as in the previous embodiments. Alternatively, however, it may also coincide approximately with the dashed line characterizing the flow of the carrier gas 8 in FIG.
- the coil surrounds the quartz glass container, not shown, with the containers 2, 2a arranged therein horizontally in the illustration and transversely to the viewing direction.
- the apparatus according to the fourth embodiment is not limited to the geometry of the dual-chamber crucible system shown in FIG.
- Other container and channel geometries as well as possibly several channels are also possible, provided that the laminar character of the gas flow of the carrier gas 8 (or of the carrier gas mixture) is retained.
- the device according to the fourth embodiment is further not limited to the use of a carrier gas.
- the evaporation of the molten metal in a high vacuum is also possible.
- the heating of the crucible system up to the setting of a defined partial pressure of the species evaporated from the molten metal 6 corresponds to the principles described in detail in the second exemplary embodiment (FIGS. 2, 3).
- the statements made for the second exemplary embodiment for selecting the materials 5, 6 as well as for the crucible elements also apply without restriction to the fourth exemplary embodiment described here.
Abstract
Description
Claims
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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PL12791755T PL2622112T3 (pl) | 2011-12-21 | 2012-11-27 | Urządzenie i sposób odparowywania materiału ze stopionej masy metalicznej |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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DE102011089501A DE102011089501B4 (de) | 2011-12-21 | 2011-12-21 | Vorrichtung und Verfahren zum Verdampfen von Material aus einer Metallschmelze |
PCT/EP2012/073677 WO2013092124A1 (de) | 2011-12-21 | 2012-11-27 | Vorrichtung und verfahren zum verdampfen von material aus einer metallschmelze |
Publications (2)
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EP2622112A1 true EP2622112A1 (de) | 2013-08-07 |
EP2622112B1 EP2622112B1 (de) | 2015-01-07 |
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EP12791755.7A Active EP2622112B1 (de) | 2011-12-21 | 2012-11-27 | Vorrichtung und verfahren zum verdampfen von material aus einer metallschmelze |
Country Status (5)
Country | Link |
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US (1) | US10767255B2 (de) |
EP (1) | EP2622112B1 (de) |
DE (1) | DE102011089501B4 (de) |
PL (1) | PL2622112T3 (de) |
WO (1) | WO2013092124A1 (de) |
Families Citing this family (7)
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DE102013108997A1 (de) * | 2013-08-20 | 2015-02-26 | Von Ardenne Gmbh | Tiegelanordnung und Vakuumbeschichtungsanlage |
DE102013224319A1 (de) * | 2013-11-27 | 2015-06-11 | Eos Gmbh Electro Optical Systems | Verfahren und Vorrichtung zum generativen Herstellen zumindest eines Bauteilbereichs eines Bauteils |
CN104726828B (zh) * | 2015-03-26 | 2017-06-06 | 青州市宝丰镀膜科技有限公司 | 双开式感应加热镀膜机 |
CN111278770B (zh) | 2017-10-27 | 2023-04-21 | 凯文艾伦杜利股份有限公司 | 用于制造高纯度硅的系统及方法 |
JP7018816B2 (ja) * | 2018-04-26 | 2022-02-14 | 昭和電工株式会社 | 坩堝及びSiC単結晶成長装置 |
GB2586634B (en) * | 2019-08-30 | 2022-04-20 | Dyson Technology Ltd | Multizone crucible apparatus |
DE102021200421A1 (de) | 2021-01-18 | 2022-07-21 | Alethia-Group Gmbh | Sprüheinheit und Verfahren zum Aufsprühen eines aus einem Festkörper gewonnenen Materials |
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CH564393A5 (de) * | 1973-11-05 | 1975-07-31 | Bbc Brown Boveri & Cie | |
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US3980438A (en) * | 1975-08-28 | 1976-09-14 | Arthur D. Little, Inc. | Apparatus for forming semiconductor crystals of essentially uniform diameter |
US4036595A (en) * | 1975-11-06 | 1977-07-19 | Siltec Corporation | Continuous crystal growing furnace |
US4125086A (en) * | 1977-01-06 | 1978-11-14 | The United States Of America As Represented By The Secretary Of The Army | Nozzle beam type metal vapor source |
US4352784A (en) * | 1979-05-25 | 1982-10-05 | Western Electric Company, Inc. | Double crucible Czochralski crystal growth apparatus |
US4246064A (en) * | 1979-07-02 | 1981-01-20 | Western Electric Company, Inc. | Double crucible crystal growing process |
JPS58197270A (ja) * | 1982-05-12 | 1983-11-16 | Mitsubishi Electric Corp | 蒸発源るつぼ |
US4791261A (en) | 1987-09-23 | 1988-12-13 | International Business Machines Corporation | Crucible for evaporation of metallic film |
JPH10158088A (ja) * | 1996-11-25 | 1998-06-16 | Ebara Corp | 固体材料の製造方法及びその製造装置 |
US6649888B2 (en) * | 1999-09-23 | 2003-11-18 | Codaco, Inc. | Radio frequency (RF) heating system |
US6279352B1 (en) * | 1999-12-30 | 2001-08-28 | Corning Incorporated | Long hot zone furnace element and optical fiber drawing method practiced therewith |
US6550279B1 (en) * | 2000-09-01 | 2003-04-22 | Corning Incorporated | Process for drawing optical fiber from a multiple crucible apparatus with a thermal gradient |
JP3864696B2 (ja) * | 2000-11-10 | 2007-01-10 | 株式会社デンソー | 炭化珪素単結晶の製造方法及び製造装置 |
JP2003074828A (ja) * | 2001-08-29 | 2003-03-12 | Hikari Tekku Kk | 灰の溶融装置 |
US6588235B2 (en) * | 2001-08-30 | 2003-07-08 | Corning Incorporated | Method of centering a fiber core in a multiple-crucible method |
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JP2005336558A (ja) * | 2004-05-27 | 2005-12-08 | Konica Minolta Medical & Graphic Inc | 蒸着装置及び蒸着方法 |
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US8361227B2 (en) * | 2006-09-26 | 2013-01-29 | Ii-Vi Incorporated | Silicon carbide single crystals with low boron content |
EP1967604A1 (de) * | 2007-03-08 | 2008-09-10 | Applied Materials, Inc. | Verdampfungstiegel und Verdampfungsvorrichtung mit gerichteter Verdampfung |
US7862656B2 (en) * | 2007-07-03 | 2011-01-04 | Siemens Medical Solutions Usa, Inc. | Apparatus and method for growing a crystal and heating an annular channel circumscribing the crystal |
US8784559B2 (en) * | 2010-09-09 | 2014-07-22 | Siemens Medical Solutions Usa, Inc. | Method and apparatus for continuous crystal growth |
-
2011
- 2011-12-21 DE DE102011089501A patent/DE102011089501B4/de active Active
-
2012
- 2012-11-27 PL PL12791755T patent/PL2622112T3/pl unknown
- 2012-11-27 EP EP12791755.7A patent/EP2622112B1/de active Active
- 2012-11-27 WO PCT/EP2012/073677 patent/WO2013092124A1/de active Application Filing
- 2012-12-20 US US13/721,086 patent/US10767255B2/en active Active
Non-Patent Citations (1)
Title |
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See references of WO2013092124A1 * |
Also Published As
Publication number | Publication date |
---|---|
EP2622112B1 (de) | 2015-01-07 |
PL2622112T3 (pl) | 2015-06-30 |
DE102011089501B4 (de) | 2013-10-10 |
US20130163967A1 (en) | 2013-06-27 |
DE102011089501A1 (de) | 2013-06-27 |
US10767255B2 (en) | 2020-09-08 |
WO2013092124A1 (de) | 2013-06-27 |
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